U.S. patent application number 14/381743 was filed with the patent office on 2015-02-26 for extrusion process.
The applicant listed for this patent is DSM IP ASSETS B.V.. Invention is credited to Petrus Henricus Maria Elemans, Bruno Leuenberger, Adrian Willem Meesen, Alexandra Teleki.
Application Number | 20150056345 14/381743 |
Document ID | / |
Family ID | 47749855 |
Filed Date | 2015-02-26 |
United States Patent
Application |
20150056345 |
Kind Code |
A1 |
Elemans; Petrus Henricus Maria ;
et al. |
February 26, 2015 |
EXTRUSION PROCESS
Abstract
The present invention relates to a process for the production of
extruded formulations (=extrudates) comprising dispersion droplets,
to such formulations as well as to the use of such formulations in
food, feed, personal care applications.
Inventors: |
Elemans; Petrus Henricus Maria;
(Basel, CH) ; Meesen; Adrian Willem; (Basel,
CH) ; Teleki; Alexandra; (Basel, CH) ;
Leuenberger; Bruno; (Basel, CH) |
|
Applicant: |
Name |
City |
State |
Country |
Type |
DSM IP ASSETS B.V. |
Heerlen |
|
NL |
|
|
Family ID: |
47749855 |
Appl. No.: |
14/381743 |
Filed: |
February 27, 2013 |
PCT Filed: |
February 27, 2013 |
PCT NO: |
PCT/EP2013/053843 |
371 Date: |
August 28, 2014 |
Current U.S.
Class: |
426/250 ;
426/540 |
Current CPC
Class: |
A23D 7/04 20130101; A23K
20/10 20160501; A23K 20/158 20160501; A23K 40/20 20160501; A23D
7/0053 20130101; A23K 20/179 20160501; A23K 20/163 20160501; A23V
2002/00 20130101; A23L 27/70 20160801; A23K 20/174 20160501; A61K
8/31 20130101; A23L 5/44 20160801; A23L 33/15 20160801; A23V
2002/00 20130101; A23K 20/147 20160501; A23P 30/20 20160801; A23K
40/25 20160501; A61Q 19/00 20130101; A23V 2200/222 20130101; A23V
2250/211 20130101; A23V 2300/16 20130101; A23V 2250/5118 20130101;
A23L 29/212 20160801; A23V 2200/224 20130101 |
Class at
Publication: |
426/250 ;
426/540 |
International
Class: |
A23L 1/275 20060101
A23L001/275 |
Foreign Application Data
Date |
Code |
Application Number |
Feb 28, 2012 |
EP |
12157279.6 |
Claims
1. Process of production of an extrudate, wherein that extrudate
comprises dispersion droplets and wherein these dispersion droplets
comprise at least one carotenoid and at least one emulsifying
protective colloid and water, characterised in that the dispersion
process is carried out in the extruder.
2. Process according to claim 1, wherein the process is carried out
without an organic solvent.
3. Process according to claim 1, wherein the carotenoid is chosen
from the group consisting of -carotene, .cndot.-carotene,
8'-apo-.cndot.-carotenal, 8'-apo--carotenoic acid esters such as
the ethyl ester, canthaxanthin, astaxanthin, lycopene, lutein,
zeaxanthin and crocetin.
4. Process according to claim 1, wherein the carotenoid is
.cndot.-carotene.
5. Process according to claim 1, wherein the emulsifying protective
colloid is chosen from the group consisting of modified (food)
starches, ascorbyl palmitate, pectin, alginate, carrageenan,
furcellaran, dextrin derivatives, celluloses and cellulose
derivatives (e.g. cellulose acetate, methyl cellulose,
hydroxypropyl methyl cellulose), lignosulfonate, polysaccharide
gums (such as gum acacia, xanthan gum, flaxseed gum, ghatti gum,
tamarind gum and arabinogalactan), gelatine (bovine, fish, pork,
poultry), plant proteins (such as are for example peas, soybeans,
castor beans, cotton, potatoes, sweet potatoes, manioc, rapeseed,
sunflowers, sesame, linseed, safflower, lentils, nuts, wheat, rice,
maize, barley, rye, oats, lupin and sorghum), animal proteins
including milk or whey proteins, lecithin, polyglycerol ester of
fatty acids, monoglycerides of fatty acids, diglycerides of fatty
acids, sorbitan ester, PG ester and sugar ester (as well as
derivatives thereof).
6. Process according to claim 1, wherein 0.5 wt-%-50 wt-%,
preferably 1 wt-%-30 wt-%, based on the total weight of the
extrudate, of at least one carotenoid is used.
7. Process according to claim 1, wherein 5 wt-%-80 wt-%, preferably
15 wt-%-80 wt-%, more preferably 30 wt-% to 80 wt-%, based on the
total weight of the extrudate, of at least one emulsifying
protective colloid is used.
8. Process according to claim 1, wherein 1 wt-%-90 wt-%, preferably
1 wt-%-80 wt-%, more preferably 1 wt-%-60 wt-%, based on the total
weight of the extrudate, of water is used.
9. Process according to claim 1, wherein 5 wt-%-30 wt-%, based on
the total weight of the extrudate, of water is used.
10. Process according to claim 1, wherein 0.1 wt-%-50 wt-%, based
on the total weight of the extrudate, of at least one auxiliary
agent is used.
11. Process according to claim 10, wherein the auxiliary agent is
chosen from the group consisting of antioxidants (such as ascorbic
acid or salts thereof, tocopherol (synthetic or natural); butylated
hydroxytoluene (BHT); butylated hydroxyanisole (BHA); propyl
gallate; tert. butyl hydroxyquinoline and/or ascorbic acid esters
of a fatty acid); ethoxyquin, plasticisers, stabilisers, humectants
(such as glycerine, sorbitol, polyethylene glycol) protective
colloids without emulsifying properties, gelling agents (such as
chitosan), dyes, fragrances, fillers (such as maltodextrin) and
buffers.
12. Process according to claim 1, wherein the emulsifying
protective colloid (or a mixture of emulsifying protective
colloids) is added first, then the water and then afterwards the
carotenoid.
13. Process according to claim 1, wherein the carotenoid is
.cndot.-carotene and wherein the .cndot.-carotene is added to the
process at the beginning and in liquid (molten) form.
14. Process according to claim 1, wherein the carotenoid is
.cndot.-carotene and wherein the .cndot.-carotene is added to the
process as a pure powder or in a mixture with at least one modified
(food) starch either at the beginning of the process or at any
stage later.
15. Process according to claim 1, wherein the temperature inside
the extruder is between 20.degree. C. and 220.degree. C.
16. Process according to claim 1, wherein the total residence time
for the ingredients is between 1 and 400 s.
17. Extrudates comprising dispersion droplets, wherein these
dispersion droplets comprise at least one carotenoid and at least
one emulsifying protective colloid, and water, and optionally at
least one auxiliary agent.
18. Extrudates according to claim 17, wherein the average particle
size of the dispersion droplets are less than 1000 nm (preferably
the average particle size of the dispersion droplets is between 50
nm and 500 nm, more preferably 100 nm-300 nm).
19. Extrudates according to claim 17 comprising 0.5 wt-%-50 wt-%,
based on the total weight of the extrudate, of at least one
carotenoid, and 5 wt-%-80 wt-%, based on the total weight of the
extrudate, of at least one emulsifying protective colloid, and 1
wt-%-90 wt-%, based on the total weight of the extrudate, of water,
and optionally 0.1 wt-%-50 wt-%, based on the total weight of the
extrudate, of at least one auxiliary agent.
20. Extrudates according to claim 17 comprising 1 wt-%-30 wt-%,
preferably 1 wt-%-20 wt-%,based on the total weight of the
extrudate, of at least one based on the total weight of the
extrudate, of at least one carotenoid chosen from the group
consisting of .cndot.-carotene, .cndot.-carotene,
8'-apo-.cndot.-carotenal, 8'-apo-.cndot.-carotenoic acid esters
such as the ethyl ester, canthaxanthin, astaxanthin, lycopene,
lutein, zeaxanthin and crocetin (preferred is
.cndot.-carotene).
21. Extrudates according to claim 17 comprising 15 wt-%-80 wt-%,
preferably 30 wt-%-80 wt-%, based on the total weight of the
extrudate, of at least one emulsifying protective colloid, wherein
the emulsifying protective colloid is chosen from the group
consisting of modified (food) starches, ascorbyl palmitate, pectin,
alginate, carrageenan, furcellaran, dextrin derivatives, celluloses
and cellulose derivatives (e.g. cellulose acetate, methyl
cellulose, hydroxypropyl methyl cellulose), lignosulfonate,
polysaccharide gums (such as gum acacia, xanthan gum, flaxseed gum,
ghatti gum, tamarind gum and arabinogalactan), gelatine (bovine,
fish, pork, poultry), plant proteins (such as are for example peas,
soybeans, castor beans, cotton, potatoes, sweet potatoes, manioc,
rapeseed, sunflowers, sesame, linseed, safflower, lentils, nuts,
wheat, rice, maize, barley, rye, oats, lupin and sorghum), animal
proteins including milk or whey proteins, lecithin, polyglycerol
ester of fatty acids, monoglycerides of fatty acids, diglycerides
of fatty acids, sorbitan ester, PG ester and sugar ester (as well
as derivatives thereof).
22. Extrudates according to claim 17 comprising 1 wt-%-80 wt-%,
preferably 1 wt-%-60 wt-%, more preferably 5 wt-%-30 wt-%, based on
the total weight of the extrudate, of water.
23. Extrudates according to claim 17 comprising 0.1 wt-%-50 wt-%,
based on the total weight of the extrudate, of at least one
auxiliary chosen from the group consisting of antioxidants (such as
ascorbic acid or salts thereof, tocopherol (synthetic or natural);
butylated hydroxytoluene (BHT); butylated hydroxyanisole (BHA);
propyl gallate; tert. butyl hydroxyquinoline; ethoxyquin and/or
ascorbic acid esters of a fatty acid), plasticisers, stabilisers,
humectants (such as glycerine, sorbitol, polyethylene glycol)
protective colloids without emulsifying properties, gelling agents
(such as chitosan), dyes, fragrances, fillers (such as
maltodextrin) and buffers.
24. Use of an extrudate as obtained from claim 1 in a food, feed,
personal care product.
25. A food, feed, personal care product comprising at least one
extrudate as obtained from claim 1.
Description
[0001] The present invention relates to a process for the
production of extruded formulations (=extrudates) comprising
dispersion droplets, to such formulations as well as to the use of
such formulations in food, feed, personal care applications.
[0002] More precisely, the present invention relates to a process
for the production of extruded formulations comprising dispersion
droplets, wherein the dispersion comprises at least one carotenoid,
at least one emulsifying protective colloid and water.
[0003] The terms "emulsion" and "dispersion" in the context of the
present invention are synonyms. A dispersion in the context of the
present invention comprises (at least). one (or more) carotenoid
and one (or more) emulsifying protective colloid and water.
[0004] There are many ways to formulate carotenoids. The types of
formulations are depending i.e. on the use of these formulations in
the final application as well as on the kind of material
(ingredients) which are used. However, the most important and
demanding formulations are the so-called dried dispersions. The
carotenoid is emulsified into an aqueous phase containing a matrix
material and/or a suitable emulsifying protective colloid. After
drying, the carotenoid is embedded in the matrix material. It is
possible that the carotenoid is (partially) crystallised in the
extrudate.
[0005] Known technologies for dispersion are e.g.
rotor-stator-systems, high pressure homogenizers or ultrasonic
devices. A major disadvantage of these technologies is that a
relatively low viscosity (usually below 1 Pas) is required, leading
to high amounts of water in the dispersion. Usually these processes
require the use of an organic solvent which has to be removed after
dispersion or precipitation.
[0006] Extrusion processes (and extruders) are well known in the
field of formulations. They can be used for many different kinds of
materials, such as thermoplastics and rubbers, as well as food- and
feedstuffs.
[0007] The main advantages of using the extrusion technology is
that high viscous solutions can be formulated and less water can be
used for the dispersion, which then requires less drying.
Furthermore an extrusion process can be run as a continuous process
and it can be run without organic solvents.
[0008] It can be found in the prior art that emulsions comprising
fat soluble vitamins are extruded. US 2004/0201116 discloses
pellets which are obtained by a combination of producing emulsions
using devices like high pressure homogenizers with subsequent
direct pelleting or extrusion as a second process step.
[0009] The goal of the present invention was to find a way for the
production of extrudates comprising dispersion droplets, which
comprise carotenoid(s).
[0010] Carotenoids are distinctly different from lipophilic
vitamins and lipophilic flavours. These lipophilic vitamins are
either liquid or can easily be made liquid by using reasonable
temperatures well below 100.degree. C. Carotenoids are lipophilic,
cannot be melted around 100.degree. C., and decompose at higher
temperatures. They are classical representative of the so-called
sparingly soluble lipophilic actives.
[0011] A new way for the production of such extrudates was found.
Surprisingly it was found out that when the dispersion process is
carried out inside the extruder, the process as well as the
obtained extrudates are improved.
[0012] When the dispersion process is carried out in the extruder
(extrudation apparatus), this results in extrudates, wherein [0013]
(i) very small average dispersion droplets sizes can be obtained,
and [0014] (ii) a very narrow and monomodal distribution of the
droplet sizes is obtained, and [0015] (iii) such a process can
easily be run as a continuous process, and [0016] (iv) no organic
solvent is used and [0017] (v) less water can be used and therefore
less energy for drying the extrudate is necessary.
[0018] Therefore the present invention relates to a process of
production of an extrudate, wherein that extrudate comprises
dispersion droplets, wherein these dispersion droplets comprise at
least one carotenoid and at least one emulsifying protective
colloid and water, characterised in that the emulsifying process is
carried out in the extruder.
[0019] The term "carotenoid" as used herein comprises a natural or
synthetic carotene or structurally related polyene compound which
can be used as a functional health ingredient or colorant for food,
such as .alpha.- or .beta.-carotene, 8'-apo-.beta.-carotenal,
8'-apo-.beta.-carotenoic acid esters such as the ethyl ester,
canthaxanthin, astaxanthin, lycopene, lutein, zeaxanthin or
crocetin, or mixtures thereof. The preferred carotenoids are
.beta.-carotene, lycopene and lutein and mixtures thereof,
especially .beta.-carotene.
[0020] Therefore a preferred embodiment of the present invention is
a process as described above, wherein the one or more carotenoid is
chosen from the group consisting of .alpha.-carotene,
.beta.-carotene, 8'-apo-.beta.-carotenal, 8'-apo-.beta.-carotenoic
acid esters such as the ethyl ester, canthaxanthin, astaxanthin,
lycopene, lutein, zeaxanthin and crocetin.
[0021] In an especially preferred process the carotenoid is
.beta.-carotene.
[0022] At least one emulsifying protective colloid is used in the
process according to the present invention. The term emulsifying
protective colloid covers all protective colloids having
emulsifying properties. Any commonly known and used emulsifying
protective colloid can be used. The emulsifying protective colloid
can be chosen depending on the final use of the extrudate
afterwards. That means if the extrudate obtained by the process
according to the present invention is used in food or feed
products, the emulsifying protective colloid must be food or feed
grade.
[0023] Suitable emulsifying protective colloids are i.e. modified
(food) starches, ascorbyl palmitate, pectin, alginate, carrageenan,
furcellaran, dextrin derivatives, celluloses and cellulose
derivatives (e.g. cellulose acetate, methyl cellulose,
hydroxypropyl methyl cellulose), lignosulfonate, polysaccharide
gums (such as gum acacia (=gum arabic), xanthan gum, flaxseed gum,
ghatti gum, tamarind gum and arabinogalactan), gelatine (bovine,
fish, pork, poultry), plant proteins (such as are for example peas,
soybeans, castor beans, cotton, potatoes, sweet potatoes, manioc,
rapeseed, sunflowers, sesame, linseed, safflower, lentils, nuts,
wheat, rice, maize, barley, rye, oats, lupin and sorghum), animal
proteins including milk or whey proteins, lecithin, polyglycerol
ester of fatty acids, monoglycerides of fatty acids, diglycerides
of fatty acids, sorbitan ester, PG ester and sugar ester (as well
as derivatives thereof).
[0024] The starches can be modified physically and chemically.
Pregelatinized starches are examples of physically modified
starches. Acidic modified, oxidized, cross-linked, starch esters,
starch ethers and cationic starches are examples of chemically
modified starches.
[0025] A preferred embodiment therefore relates to a process,
wherein at least one emulsifying protective colloid is chosen from
the group consisting of modified (food) starches, ascorbyl
palmitate, pectin, alginate, carrageenan, furcellaran, dextrin
derivatives, celluloses and cellulose derivatives (e.g. cellulose
acetate, methyl cellulose, hydroxypropyl methyl cellulose),
lignosulfonate, polysaccharide gums (such as gum acacia (=gum
arabic), xanthan gum, flaxseed gum, ghatti gum, tamarind gum and
arabinogalactan), gelatine (bovine, fish, pork, poultry), plant
proteins (such as are for example peas, soybeans, castor beans,
cotton, potatoes, sweet potatoes, manioc, rapeseed, sunflowers,
sesame, linseed, safflower, lentils, nuts, wheat, rice, maize,
barley, rye, oats, lupin and sorghum), animal proteins including
milk or whey proteins, lecithin, polyglycerol ester of fatty acids,
monoglycerides of fatty acids, diglycerides of fatty acids,
sorbitan ester, PG ester and sugar ester (as well as derivatives
thereof).
[0026] Water is also used in the process according to the present
invention.
[0027] It is also possible to add further ingredients (auxiliary
agents) during the process of formulation (extrudation). Such
auxiliary agents can be useful for the extrusion process and/or for
the extrudate and/or for the product (or application), wherein the
extrudate is used afterwards.
[0028] Such auxiliary agents are for example antioxidants (such as
ascorbic acid or salts thereof, tocopherols (synthetic or natural);
butylated hydroxytoluene (BHT); butylated hydroxyanisole (BHA);
propyl gallate; tert. butyl hydroxyquinoline and/or ascorbic acid
esters of a fatty acid); ethoxyquin, plasticisers, stabilisers,
humectants (such as glycerine, sorbitol, polyethylene glycol)
protective colloids without emulsifying properties, gelling agents
(such as chitosan), dyes, fragrances, fillers (such as
maltodextrin) and buffers.
[0029] These auxiliary agents are added optionally. When added then
the amount of the auxiliary agents goes from 0.1 to 50 weight-%
(wt-%), based on the total weight of the extrudate.
[0030] The extrudates obtained by the process according to the
present invention comprise: [0031] 0.5 wt-%-50 wt-%, based on the
total weight of the extrudate, of at least one carotenoid, and
[0032] 5 wt-%-80 wt-%, based on the total weight of the extrudate,
of at least one emulsifying protective colloid, and [0033] 1
wt-%-90 wt-%, based on the total weight of the extrudate, of water,
and optionally [0034] 0.1 wt-%-50 wt-%, based on the total weight
of the extrudate, of at least one auxiliary agent.
[0035] All the percentages always add up to 100.
[0036] All the preferences listed above for the carotenoids, the
emulsifying protective colloids and the auxiliary agents also apply
to the composition of the extrudate.
[0037] Preferably 1 wt-%-45 wt-%, based on the total weight of the
extrudate, of at least one carotenoid is used. More preferably 1
wt-%-30 wt-%, especially preferred 1 wt-%-20 wt-%, most preferred 1
wt-%-15 wt-%, based on the total weight of the extrudate, of at
least one carotenoid is used.
[0038] Preferably 15 wt-%-80 wt-%, more preferably 30 wt-%-80 wt-%,
most preferably 50 wt-%-80 wt-%, based on the total weight of the
extrudate, of at least one emulsifying protective colloid is
used.
[0039] Preferably 1 wt-%-80 wt-%, more preferably 1 wt-%-60 wt-%,
based on the total weight of the extrudate, of water is used. As
already mentioned above, it also possible to use a low amount of
water. Therefore 5 wt-%-30 wt-%, based on the total weight of the
extrudate, of water can be used. Such a low amount of water cannot
be used when an extrudate is produced by adding the dispersion into
the extruder.
[0040] For the modified food starches the water content is
preferably 10 wt-%-30 wt-%, based on the total weight of the
extrudate.
[0041] One of the advantages of the present invention is that the
size distribution of the average droplet sizes of the dispersion
inside the extrudate is narrow and monomodal. This means that the
carotenoid is nearly homogenously distributed inside the extrudate,
which allows afterwards very precise dosages.
[0042] It is also possible (but not essential) that the dispersion
can be filtered before the extrusion process.
[0043] Furthermore, the process according to the present invention
allows to producing very small sized droplets inside the extrudate.
The average droplet size can be as small as 50 nm. Usually the
droplets are smaller than 1 .mu.m.
[0044] Preferably the average droplet (d.sub.3,2) is between 50 nm
and 1000 nm.
[0045] The droplet sizes are measured by using commonly known and
standardized methods. Suitable methods are light scattering or
laser diffraction. The given values of the droplet sizes are always
(d.sub.3,2).
[0046] More preferably the average droplet (d.sub.3,2) is between
50 nm and 500 nm, especially preferred 100-300 nm.
[0047] The extrusion process is characterised in that the
dispersion is carried out inside the extruder. Usually the three
main ingredients (carotenoid and emulsifying protective colloid and
water) are added at different inlets of the extruder process. These
inlets are arranged separated from each other. When (optionally)
auxiliary agents are added, they can be added together with one or
more of the main ingredients or they can also be added in a
separate step.
[0048] Usually the emulsifying protective colloid is added first,
then the water and then the carotenoid is added. It is also
possible that one ingredient is added through more than one inlet
of the extruder at different locations. Therefore a further
embodiment of the present invention relates to a process, wherein
the emulsifying protective colloid (or a mixture of emulsifying
protective colloids) is added first, then the water and then
afterwards the carotenoid (or a mixture of carotenoids).
[0049] A preferred embodiment of the present invention relates to a
process wherein the carotenoid is .beta.-carotene. In this case
.beta.-carotene is either added [0050] (i) as a liquid (molten)
into the extruder, or [0051] (ii) as a solid powder (optionally
premixed with at least one modified (food) starch and wherein the
powder can be added to the process at the start of the extruder or
at any stage).
[0052] The temperature inside the extruder is usually between 20
and 220.degree. C. Preferably the temperature of extrudate exiting
the extruder is <100.degree. C. The total residence time for the
ingredients in the extruder is usually between 1 and 400 s.
[0053] The amount of shear of the extrudation process according to
the present invention is usually 100 to 200000 units.
[0054] Furthermore, it is also possible to pump inert gas through
the extruder. The inert gas is usually pumped in at the entrance of
the extruder. But it could also be pumped in at any stage of the
extrusion process (also through several inlets at different
locations). Inert gas can be helpful to protect sensible
ingredients.
[0055] The extruder comprises usually one or more screw shafts on
which various conveying or kneading type screw elements are
mounted.
[0056] The material is transported by these elements through the
extruder (optionally under pressure and elevated temperature). At
the end (exit) of the extruder there can be a die through which the
extruded material is pressed. Afterwards the extruded material is
dried and cut (or also vice versa). The extruder can have several
inlets through which the material can be added.
[0057] In the case of the present invention there are several
inlets to add the emulsifying protective colloid(s), the
carotenoid(s), water and optionally the auxiliary agents.
[0058] A further embodiment of the present invention relates to new
extrudates. These inventive extrudates comprise dispersion droplets
which have a very small average droplet size, and wherein the
distribution of the droplet sizes is narrow and monomodal.
[0059] Therefore a further embodiment of the present invention
relates to extrudates comprising dispersion droplets, wherein these
dispersion droplets comprise [0060] at least one carotenoid and
[0061] at least one emulsifying protective colloid, and [0062]
water, and optionally [0063] at least one auxiliary agent.
[0064] A preferred embodiment of the present invention relates to
extrudates comprising dispersion droplets, wherein these dispersion
droplets comprise [0065] at least one carotenoid and [0066] at
least one emulsifying protective colloid, and [0067] water, and
optionally [0068] at least one auxiliary agent, [0069]
characterised in that the average particle size of the dispersion
droplets are less than 1000 nm (preferably the average particle
size of the dispersion droplets is between 50 nm and 500 nm, more
preferably 100 nm-300 nm).
[0070] The average particle size of the dispersion droplets are
measured by laser diffraction with a Malvern Mastersizer 2000 and
Hydro 2000 S sample dispersion unit. The average particle size of
the dispersion droplets can also be determined by dynamic light
scattering, e.g. with a Malvern Zetasizer Nano.
[0071] It is possible that in the extrudate some of the carotenoid
is crystallised (precipitated), due to the solubility of the
carotenoids in oil.
[0072] Preferred extrudates according to the present invention
comprise: [0073] 0.5 wt-%-50 wt-%, based on the total weight of the
extrudate, of at least one carotenoid, and [0074] 5 wt-%-90 wt-%,
based on the total weight of the extrudate, of at least one
emulsifying protective colloid, and [0075] 1 wt-%-80 wt-%, based on
the total weight of the extrudate, of water and optionally [0076]
0.1 wt-%-50 wt-%, based on the total weight of the extrudate, of at
least one auxiliary agent, [0077] characterised in that the average
particle size of the dispersion droplets are less than 1000 nm
(preferably the average particle size of the dispersion droplets is
between 50 nm and 500 nm, more preferably 100 nm-300 nm).
[0078] More preferred are extrudates comprising [0079] 1 wt-%-30
wt-%, based on the total weight of the extrudate, of at least one
carotenoid chosen from the group consisting of .alpha.-carotene,
.beta.-carotene, 8'-apo-.beta.-carotenal, 8'-apo-.beta.-carotenoic
acid esters such as the ethyl ester, canthaxanthin, astaxanthin,
lycopene, lutein, zeaxanthin and crocetin (most preferred is
.beta.-carotene), and [0080] 15 wt-%-80 wt-%, based on the total
weight of the extrudate, of at least one emulsifying protective
colloid, wherein the emulsifying protective colloid is chosen from
the group consisting of modified (food) starches, ascorbyl
palmitate, pectin, alginate, carrageenan, furcellaran, dextrin
derivatives, celluloses and cellulose derivatives (e.g. cellulose
acetate, methyl cellulose, hydroxypropyl methyl cellulose),
lignosulfonate, polysaccharide gums (such as gum acacia, xanthan
gum, flaxseed gum, ghatti gum, tamarind gum and arabinogalactan),
gelatine (bovine, fish, pork, poultry), plant proteins (such as are
for example peas, soybeans, castor beans, cotton, potatoes, sweet
potatoes, manioc, rapeseed, sunflowers, sesame, linseed, safflower,
lentils, nuts, wheat, rice, maize, barley, rye, oats, lupin and
sorghum), animal proteins including milk or whey proteins,
lecithin, polyglycerol ester of fatty acids, monoglycerides of
fatty acids, diglycerides of fatty acids, sorbitan ester, PG ester
and sugar ester (as well as derivatives thereof), and [0081] 1
wt-%-60 wt-%, based on the total weight of the extrudate, of water,
and optionally [0082] 0.1 wt-%-50 wt-%, based on the total weight
of the extrudate, of at least one auxiliary agent, wherein the
auxiliary agent is chosen from the group consisting of antioxidants
(such as ascorbic acid or salts thereof, tocopherol (synthetic or
natural); butylated hydroxytoluene (BHT); butylated hydroxyanisole
(BHA); propyl gallate; tert. butyl hydroxyquinoline and/or ascorbic
acid esters of a fatty acid); ethoxyquin, plasticisers,
stabilisers, humectants (such as glycerine, sorbitol, polyethylene
glycol) protective colloids without emulsifying properties, gelling
agents (such as chitosan), dyes, fragrances, fillers (such as
maltodextrin) and buffers. [0083] characterised in that the average
particle size of the dispersion droplets are less than 1000 nm
(preferably the average particle size of the dispersion droplets is
between 50 nm and 500 nm, more preferably 100 nm-300 nm).
[0084] Also more preferred are extrudates comprising [0085] 1
wt-%-20 wt-%, based on the total weight of the extrudate, of at
least one carotenoid chosen from the group consisting of
.alpha.-carotene, .beta.-carotene, 8'-apo-.beta.-carotenal,
8'-apo-.beta.-carotenoic acid esters such as the ethyl ester,
canthaxanthin, astaxanthin, lycopene, lutein, zeaxanthin and
crocetin (most preferred is .beta.-carotene), and [0086] 15 wt-%-80
wt-%, based on the total weight of the extrudate, of at least one
emulsifying protective colloid, wherein the emulsifying protective
colloid is chosen from the group consisting of modified (food)
starches, ascorbyl palmitate, pectin, alginate, carrageenan,
furcellaran, dextrin derivatives, celluloses and cellulose
derivatives (e.g. cellulose acetate, methyl cellulose,
hydroxypropyl methyl cellulose), lignosulfonate, polysaccharide
gums (such as gum acacia, xanthan gum, flaxseed gum, ghatti gum,
tamarind gum and arabinogalactan), gelatine (bovine, fish, pork,
poultry), plant proteins (such as are for example peas, soybeans,
castor beans, cotton, potatoes, sweet potatoes, manioc, rapeseed,
sunflowers, sesame, linseed, safflower, lentils, nuts, wheat, rice,
maize, barley, rye, oats, lupin and sorghum), animal proteins
including milk or whey proteins, lecithin, polyglycerol ester of
fatty acids, monoglycerides of fatty acids, diglycerides of fatty
acids, sorbitan ester, PG ester and sugar ester (as well as
derivatives thereof), and [0087] 5 wt-%-30 wt-%, based on the total
weight of the extrudate, of water, and optionally [0088] 0.1
wt-%-50 wt-%, based on the total weight of the extrudate, of at
least one auxiliary agent, wherein the auxiliary agent is chosen
from the group consisting of antioxidants (such as ascorbic acid or
salts thereof, tocopherol (synthetic or natural); butylated
hydroxytoluene (BHT); butylated hydroxyanisole (BHA); propyl
gallate; tert. butyl hydroxyquinoline and/or ascorbic acid esters
of a fatty acid); ethoxyquin, plasticisers, stabilisers, humectants
(such as glycerine, sorbitol, polyethylene glycol) protective
colloids, dyes, fragrances, fillers (such as maltodextrin),
protective and buffers, [0089] characterised in that the average
particle size of the dispersion droplets is less than 500 nm
(preferably the average particle size of the dispersion droplets is
between 50 nm and 300 nm).
[0090] Especially preferred are extrudates comprising [0091] 1
wt-%-20 wt-%, based on the total weight of the extrudate, of
.beta.-carotene, and [0092] 50 wt-%-80 wt-%, based on the total
weight of the extrudate, of modified (food) starches, and [0093] 10
wt-%-30 wt-%, based on the total weight of the extrudate, of water,
and optionally [0094] 0.1 wt-%-50 wt-%, based on the total weight
of the extrudate, of at least one auxiliary agent, wherein the
auxiliary agent is chosen from the group consisting of antioxidants
(such as ascorbic acid or salts thereof, tocopherol (synthetic or
natural); butylated hydroxytoluene (BHT); butylated hydroxyanisole
(BHA); propyl gallate; tert. butyl hydroxyquinoline and/or ascorbic
acid esters of a fatty acid); ethoxyquin, plasticisers,
stabilisers, humectants (such as glycerine, sorbitol, polyethylene
glycol) protective colloids, dyes, fragrances, fillers and buffers,
[0095] characterised in that the average particle size of the
dispersion droplets is less than 500 nm (preferably the average
particle size of the dispersion droplets is between 50 nm and 300
nm).
[0096] The extrudates as obtained by the process as described above
can be used in many fields of applications. Preferably the
extrudates as disclosed and described above are used in food, feed
and personal care products.
[0097] Therefore a further embodiment of the present invention
relates to the use of the extrudates as disclosed and described
above in food, feed and/or personal care products. It is to be
mentioned that dietary supplements are part of our definition of
food products.
[0098] A further embodiment of the present invention relates to
food, feed or personal care products comprising at least one of the
extrudates as disclosed and described above.
[0099] The following Examples serve to illustrate the invention.
All percentages and parts (if not otherwise indicated) are related
to the weight. The temperature is given (if not otherwise
indicated) in degree Celsius.
EXAMPLES
Example 1
Dispersion of .beta.-carotene in Modified Food Starch
[0100] The extrusion dispersion of .beta.-carotene in 10.5 g
modified food starch was conducted on a laboratory-scale conical
twin-screw (batch) extruder (DSM Xplore 15 ml micro-compounder).
10.5 g of modified food starch (HICAP 100, National Starch), was
mixed with 0.75 g of .beta.-carotene (DSM Nutritional Products) and
3.75 g demineralized water. The extruder was operated at a screw
speed of 120 rpm and a barrel temperature of 200.degree. C. The
feed hopper and extruder were purged with nitrogen. The mixture was
placed in the feed hopper and allowed to pass once through the
extruder.
[0101] The obtained extrudate was partly soluble in water resulting
in an orange, cloudy solution stable over 12 hours. This solution
was filtered either with a folded filter paper (grade 5971/2: 5-7
.mu.m) or a syringe driven filter unit (0.22 .mu.m). Filtration
with the larger pores resulted in a turbid, light-yellow solution,
while the solution from the fine filter was clear. The hydrodynamic
droplet size in these solutions was measured by dynamic light
scattering (Malvern Zetasizer). The average droplet size
(Z-Average) in the clear solution was 184 nm, while the turbid
solution also contained some larger droplets/particles resulting in
a Z-Average of 625 nm.
* * * * *